CN215310304U - Crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole - Google Patents
Crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole Download PDFInfo
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- CN215310304U CN215310304U CN202121332066.2U CN202121332066U CN215310304U CN 215310304 U CN215310304 U CN 215310304U CN 202121332066 U CN202121332066 U CN 202121332066U CN 215310304 U CN215310304 U CN 215310304U
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Abstract
The utility model discloses a crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole, which comprises a support frame, a dissolving kettle, a feeding and discharging heat exchanger, a cooler, a crystallization kettle and a storage tank, wherein the support frame is arranged on the support frame; the dissolving kettle and the crystallization kettle respectively comprise an inner barrel, an upper cover and an outer barrel; a sandwich cavity is arranged between the outer barrel and the inner barrel; a motor connected with the stirring device is arranged outside the upper cover; the charging and discharging heat exchanger and the cooler both comprise a shell and a serpentine coil; a feeding pipe is covered on the dissolving kettle; the bottom of the dissolving kettle is provided with a hot solution outlet pipe; a discharge pipe is arranged at the bottom of the crystallization kettle; a steam outlet pipe is arranged on the upper cover of the dissolving kettle; a condensed material outlet pipe is arranged at the lower part of the feeding and discharging heat exchanger; a shell of the charging and discharging heat exchanger is communicated with the upper part of the serpentine coil of the cooler, and an outlet at the lower part of the serpentine coil of the cooler is communicated with the storage tank; the cooler is provided with a cooling material outlet pipe and a cooling material inlet pipe; the upper part of the snakelike coil pipe of the feeding and discharging heat exchanger is communicated with the inner barrel of the dissolving kettle.
Description
Technical Field
The utility model belongs to the technical field of chemical production equipment, and particularly relates to a crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole.
Background
3-bromo-9- (4-biphenyl) carbazole is a chemical product produced by taking 4-bromobiphenyl and 3-bromocarbazole as raw materials. The product needs to be crystallized and purified in the production process. In the prior art, a solvent is required to be added to completely dissolve a crude product during crystallization operation, and then the temperature is reduced, so that crystals are separated out to complete the whole crystallization process. However, in the existing crystallization device, the dissolution operation and the crystallization operation are generally operated in one reaction kettle, the temperature needs to be raised and then lowered, and after the temperature is raised and dissolved, the whole temperature lowering operation needs longer time, so that the efficiency of the whole crystallization process is low; in addition, when the temperature is raised, the solvent is volatilized, the condensed solvent is directly returned to the reaction kettle, the internal fluctuation of the reaction kettle is easily caused, the temperature distribution in the whole kettle is uneven, the heat of steam condensation is not fully utilized, and the heat energy loss is large. It is therefore highly desirable to provide a crystallization apparatus for producing 3-bromo-9- (4-biphenylyl) carbazole to overcome the above problems.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problems, the utility model adopts the following technical scheme: a crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole comprises a support frame, a dissolving kettle arranged above the support frame and a crystallization kettle arranged below the support frame; the dissolving kettle and the crystallization kettle respectively comprise an inner barrel, an upper cover arranged on the inner barrel and an outer barrel sleeved outside the inner barrel; a sandwich cavity is arranged between the outer barrel and the inner barrel; a medium outlet pipe and a medium inlet pipe which are communicated with the interlayer cavity are respectively arranged above and below the outer barrel; the central part of the outer side of the upper cover is provided with a motor, and the output end of the motor is connected with a stirring device arranged in the inner barrel; a feeding pipe is arranged on the upper cover of the dissolving kettle; the bottom of the dissolving kettle is provided with a hot solution outlet pipe for communicating an inner barrel of the dissolving kettle with an inner barrel of the crystallization kettle; a discharge pipe is arranged at the central part of the bottom of the crystallization kettle; the upper cover of the dissolving kettle is provided with an inner barrel for communicating the dissolving kettle and a steam outlet pipe of a reflux system.
Further, the reflux system comprises a feeding and discharging heat exchanger and a cooler which are arranged above the support frame, and a storage tank which is arranged below the support frame; the feeding and discharging heat exchanger and the cooler respectively comprise a shell and a serpentine coil arranged in the shell; the steam outlet pipe is communicated with the upper part of the shell of the charging and discharging heat exchanger; a condensed material outlet pipe communicated with the upper part of the storage tank is arranged at the bottom of the shell of the charging and discharging heat exchanger; the middle part of the shell of the charging and discharging heat exchanger is communicated with an inlet at the upper part of the shell of the cooler, and an outlet at the bottom of the shell of the cooler is communicated with the storage tank; the upper end and the lower end of the serpentine coil of the cooler are respectively provided with a cooling material outlet pipe and a cooling material inlet pipe; the lower part of the storage tank is communicated with an inlet at the lower part of the serpentine coil of the charging and discharging heat exchanger through a liquid pump; and an outlet at the upper part of the serpentine coil of the feeding and discharging heat exchanger is communicated with an inner barrel of the dissolving kettle.
Further, the top of the cooler and the top of the storage tank are both provided with non-condensable gas outlet pipes, and the other ends of the two non-condensable gas outlet pipes are both connected with an activated carbon filter; and the two non-condensable gas outlet pipes are provided with discharge valves.
Further, the stirring device comprises a rotating shaft connected with an output shaft of the motor and a plurality of stirring blades arranged on the rotating shaft.
Furthermore, a heating wire is embedded in the stirring blade in the dissolving kettle.
Furthermore, the rotating shaft in the crystallization kettle is connected with two elastic scraping blades which are abutted against the side wall and the bottom plate of the crystallization kettle through a plurality of connecting columns, and the elastic scraping blades are symmetrically arranged along the rotating shaft in the crystallization kettle.
Furthermore, the number of the activated carbon filters is two, and inlet pipes of the activated carbon filters are respectively communicated with the non-condensable gas outlet pipe; and a switching valve is arranged on an inlet pipe of each activated carbon filter.
Furthermore, the medium outlet pipe, the medium inlet pipe, the hot solution outlet pipe, the discharge pipe, the cooling material outlet pipe and the cooling material inlet pipe are all provided with regulating valves.
The utility model has the beneficial effects that: according to the utility model, the dissolving kettle and the crystallization kettle are separately arranged, so that rapid heating and rapid cooling can be realized, and the dissolving kettle and the crystallization kettle do not interfere with each other; the utility model is provided with the feeding and discharging heat exchanger, when the condensed solvent returns to the dissolving kettle, the heat exchange can be carried out between the condensed solvent and the steam discharged from the top of the solvent kettle, so that the temperature of the solvent is not too low to influence the temperature distribution of the whole solvent kettle, and the condensed solvent is preheated by utilizing the steam, so that the heat utilization rate is higher; the non-condensable gas outlet pipe is connected with the activated carbon filter, so that harmful substances in the non-condensable gas can be adsorbed and prevented from being directly discharged into the atmosphere to pollute the environment; the utility model is provided with the elastic scraping blade, crystals can be prevented from being attached to the inner wall of the kettle body, the stirring device can effectively enhance the internal heat transfer, when the crystallized materials are discharged into the centrifugal device from the discharge pipe, the stirring device and the elastic scraping blade can also ensure that the materials are uniformly discharged from the discharge pipe, and the discharge pipe is prevented from being blocked by the deposition of solid materials.
Drawings
FIG. 1 is a schematic structural view of the present invention;
reference numerals: 1-a support frame; 2-a dissolution kettle; 3-a charge and discharge heat exchanger; 4-a cooler; 5-crystallization kettle; 6-a storage tank; 7-an activated carbon filter; 8-a liquid pump; 9-a motor; 10-a rotating shaft; 11-stirring blades; 12-heating wires; 13-upper cover; 14-inner barrel; 15-outer barrel; 16-a housing; 17-serpentine coil; 18-a cooling material outlet pipe; 19-cooling material inlet pipe; 20-a sandwich cavity; 21-an elastic blade; 22-connecting column; 23-a discharge pipe; 24-hot solution outlet pipe; 25-media outlet pipe; 26-a media inlet pipe; 27-a feed pipe; 28-a steam outlet pipe; 29-condensed material outlet pipe; 30-noncondensable gas outlet pipe.
Detailed Description
The technical solution of the present invention will be further described with reference to the accompanying drawings and examples. As shown in the attached figure 1, the crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole comprises a support frame 1, a dissolving kettle 2 arranged above the support frame 1, and a crystallization kettle 5 arranged below the support frame 1; the material inlet and outlet heat exchanger cooling system further comprises a return flow system, wherein the return flow system comprises a material inlet and outlet heat exchanger 3 and a cooler 4 which are arranged above the support frame 1, and a storage tank 6 arranged below the support frame 1.
The dissolving kettle 2 and the crystallization kettle 5 respectively comprise an inner barrel 14, an upper cover 13 arranged on the inner barrel 14 and an outer barrel 15 sleeved outside the inner barrel 14; an interlayer cavity 20 is arranged between the outer barrel 15 and the inner barrel 14; a medium outlet pipe 25 and a medium inlet pipe 26 which are communicated with the interlayer cavity 20 are respectively arranged above and below the outer barrel 15; the central part of the outer side of the upper cover 13 is provided with a motor 9, and the output end of the motor 9 is connected with a stirring device arranged in the inner barrel 1; the stirring device comprises a rotating shaft 10 connected with an output shaft of the motor 9 and a plurality of stirring blades 11 arranged on the rotating shaft 10.
The charge-discharge heat exchanger 3 and the cooler 4 each comprise a housing 16 and a serpentine 17 arranged in the housing 16. Heating wires 12 are embedded in the stirring blades 11 in the dissolving kettle 2. Set up the heater strip and can be along with stirring vane when rotating, it is more even to the inside material heating of dissolving kettle. The crystallization device is characterized in that two elastic scraping blades 21 which are abutted against the side wall and the bottom plate of the crystallization kettle 5 are connected to the rotating shaft 10 in the crystallization kettle 5 through a plurality of connecting columns 22, and the elastic scraping blades 21 are symmetrically arranged along the rotating shaft 10 in the crystallization kettle 5.
A feeding pipe 27 is arranged on the upper cover 13 of the dissolving kettle 2, a feeding hopper is arranged on the feeding pipe 27, and a sealing cover is arranged on the feeding hopper; the bottom of the dissolving kettle 2 is provided with a hot solution outlet pipe 24 for communicating the inner barrel 14 of the dissolving kettle 2 with the inner barrel 14 of the crystallization kettle 5; the crystallization kettle 5 is positioned below the dissolution kettle 2, so that materials can directly enter the crystallization kettle without a pump from the dissolution kettle to the crystallization kettle, and a middle delivery pump is omitted, so that the materials are prevented from being crystallized and blocked in the delivery process.
A discharge pipe 23 is arranged at the central part of the bottom of the crystallization kettle 5; the upper cover 13 of the dissolving kettle 2 is provided with a steam outlet pipe 28 which is used for communicating the inner barrel 14 of the dissolving kettle 2 with the upper part of the shell 16 of the charging and discharging heat exchanger 3;
the reflux system comprises a feeding and discharging heat exchanger 3 and a cooler 4 which are arranged above the support frame 1, and a storage tank 6 which is arranged below the support frame 1; the feed and discharge heat exchanger 3 and the cooler 4 each comprise a housing 16 and a serpentine coil 17 disposed within the housing 16; the steam outlet pipe 28 is communicated with the upper part of the shell 16 of the feed-discharge heat exchanger 3; a condensed material outlet pipe 29 communicated with the upper part of the storage tank 6 is arranged at the bottom of the shell 16 of the charging and discharging heat exchanger 3; the middle part of the shell 16 of the charging and discharging heat exchanger 3 is communicated with the upper part of the shell 16 of the cooler 4, and the bottom outlet of the shell 16 of the cooler 4 is communicated with the storage tank 6; the upper end and the lower end of the serpentine coil 17 of the cooler 4 are respectively provided with a cooling material outlet pipe 18 and a cooling material inlet pipe 19; the lower part of the storage tank 6 is communicated with the inlet at the lower part of the serpentine coil 17 of the charging and discharging heat exchanger 3 through a liquid pump 8; the outlet at the upper part of the serpentine coil 17 of the charging and discharging heat exchanger 3 is communicated with the inner barrel 14 of the dissolving kettle 2. The top of the cooler 4 and the top of the storage tank 6 are both provided with non-condensable gas outlet pipes 30, and the other ends of the two non-condensable gas outlet pipes 30 are both connected with an activated carbon filter 7; and two non-condensable gas outlet pipes 30 are provided with discharge valves. Be provided with two noncondensable gas outlet pipes, deposit more when leading to the heat transfer effect poor when the cooler noncondensable gas, can follow the cooler and locate the noncondensable gas emission, can follow storage jar when the noncondensable gas in the holding vessel reduces and leads to pressure great and locate the noncondensable gas emission, because the other end of noncondensable gas outlet pipe is connected with activated carbon filter can effectively prevent to cause the pollution to the atmosphere.
And regulating valves are arranged on the medium outlet pipe 25, the medium inlet pipe 26, the hot solution outlet pipe 24, the discharging pipe 23, the cooling material outlet pipe 18 and the cooling material inlet pipe 19.
The working principle is as follows: adding a material to be crystallized and a solvent into a dissolving kettle from a feeding pipe, completely dissolving the material in the solvent under the action of a heating wire and heat conducting oil introduced into a medium inlet pipe, keeping the temperature for a certain time, feeding the completely dissolved material into the crystallizing kettle from a heat solution outlet pipe for cooling and crystallizing, and discharging crystals and the solution into a centrifugal device from a discharging pipe for subsequent treatment after crystallization. Steam in the dissolving kettle enters the feeding and discharging heat exchanger through the steam outlet pipe to exchange heat with the condensed solvent, the condensed solvent is preheated, the preheated solvent returns to the dissolving kettle, the steam and the solvent enter the cooler after heat exchange, the steam is further condensed under the action of condensed water, the condensed material enters the storage tank, and non-condensable gas which cannot be condensed enters the atmosphere after being adsorbed by the activated carbon filter.
While the present invention has been described in detail with reference to the embodiments, those skilled in the art will appreciate that various changes can be made in the specific parameters of the embodiments without departing from the spirit of the present invention, and that various specific embodiments can be made, which are common variations of the present invention and will not be described in detail herein.
Claims (7)
1. A crystallization apparatus for producing 3-bromo-9- (4-biphenyl) carbazole, characterized in that: comprises a support frame (1), a dissolving kettle (2) arranged above the support frame (1) and a crystallization kettle (5) arranged below the support frame (1); the dissolving kettle (2) and the crystallization kettle (5) respectively comprise an inner barrel (14), an upper cover (13) arranged on the inner barrel (14) and an outer barrel (15) sleeved outside the inner barrel (14); an interlayer cavity (20) is arranged between the outer barrel (15) and the inner barrel (14); a medium outlet pipe (25) and a medium inlet pipe (26) which are communicated with the interlayer cavity (20) are respectively arranged above and below the outer barrel (15); a motor (9) is arranged at the central part of the outer side of the upper cover (13), and the output end of the motor (9) is connected with a stirring device arranged in the inner barrel (1); a feeding pipe (27) is arranged on the upper cover (13) of the dissolving kettle (2); the bottom of the dissolving kettle (2) is provided with a hot solution outlet pipe (24) for communicating an inner barrel (14) of the dissolving kettle (2) with an inner barrel (14) of the crystallization kettle (5); a discharge pipe (23) is arranged at the central part of the bottom of the crystallization kettle (5); an upper cover (13) of the dissolving kettle (2) is provided with an inner barrel (14) used for communicating the dissolving kettle (2) and a steam outlet pipe (28) of a reflux system.
2. A crystallization apparatus for producing 3-bromo-9- (4-biphenylyl) carbazole according to claim 1, wherein: the reflux system comprises a feeding and discharging heat exchanger (3) and a cooler (4) which are arranged above the support frame (1), and a storage tank (6) which is arranged below the support frame (1); the feed and discharge heat exchanger (3) and the cooler (4) both comprise a shell (16) and a serpentine coil (17) arranged in the shell (16); the steam outlet pipe (28) is communicated with the upper part of the shell (16) of the feeding and discharging heat exchanger (3); a condensed material outlet pipe (29) communicated with the upper part of the storage tank (6) is arranged at the bottom of the shell (16) of the feeding and discharging heat exchanger (3); the middle part of a shell (16) of the charging and discharging heat exchanger (3) is communicated with the upper part of the shell (16) of the cooler (4), and a bottom outlet of the shell (16) of the cooler (4) is communicated with the storage tank (6); the upper end and the lower end of a serpentine coil (17) of the cooler (4) are respectively provided with a cooling material outlet pipe (18) and a cooling material inlet pipe (19); the lower part of the storage tank (6) is communicated with an inlet at the lower part of a serpentine coil (17) of the charging and discharging heat exchanger (3) through a liquid pump (8); the outlet at the upper part of the serpentine coil (17) of the feeding and discharging heat exchanger (3) is communicated with the inner barrel (14) of the dissolving kettle (2).
3. A crystallization apparatus for producing 3-bromo-9- (4-biphenylyl) carbazole according to claim 2, wherein: non-condensable gas outlet pipes (30) are arranged at the top of the cooler (4) and the top of the storage tank (6), and the other ends of the two non-condensable gas outlet pipes (30) are connected with an activated carbon filter (7); and discharge valves are arranged on the two non-condensable gas outlet pipes (30).
4. A crystallization apparatus for producing 3-bromo-9- (4-biphenylyl) carbazole according to claim 1, wherein: the stirring device comprises a rotating shaft (10) connected with an output shaft of the motor (9) and a plurality of stirring blades (11) arranged on the rotating shaft (10).
5. The crystallization apparatus for producing 3-bromo-9- (4-biphenylyl) carbazole according to claim 4, wherein: heating wires (12) are embedded in the stirring blades (11) in the dissolving kettle (2).
6. A crystallization apparatus for producing 3-bromo-9- (4-biphenylyl) carbazole according to claim 1, wherein: the crystallization device is characterized in that two elastic scraping pieces (21) which are connected with the side wall of the crystallization kettle (5) and abutted against the bottom plate are connected onto a rotating shaft (10) in the crystallization kettle (5) through a plurality of connecting columns (22), and the elastic scraping pieces (21) are symmetrically arranged along the rotating shaft (10) in the crystallization kettle (5).
7. A crystallization apparatus for producing 3-bromo-9- (4-biphenylyl) carbazole according to claim 2, wherein: and regulating valves are arranged on the medium outlet pipe (25), the medium inlet pipe (26), the hot solution outlet pipe (24), the discharge pipe (23), the cooling material outlet pipe (18) and the cooling material inlet pipe (19).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121332066.2U CN215310304U (en) | 2021-06-16 | 2021-06-16 | Crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121332066.2U CN215310304U (en) | 2021-06-16 | 2021-06-16 | Crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole |
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| Publication Number | Publication Date |
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| CN215310304U true CN215310304U (en) | 2021-12-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202121332066.2U Active CN215310304U (en) | 2021-06-16 | 2021-06-16 | Crystallization device for producing 3-bromo-9- (4-biphenyl) carbazole |
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| CN (1) | CN215310304U (en) |
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2021
- 2021-06-16 CN CN202121332066.2U patent/CN215310304U/en active Active
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